Island



w. D. MDUNT, CYANID PRODUCNG APPAHATUS.

APPLICATION FILED APH, 25. !918.

Patenta-d Feb. 3; 1920.

2 SHEETS-SHEET I( INVENTOR av &aj/%Away- ATTORNEY W. D. MO'UNT.

CYAMD PRODUCING APPARATUS.

AFPLICAUON fILED APR. ?6.191E- Patented Feb. 3,1920.

2 SHEES-SHEET 2 NVENTOR TTORNEY UNITED STATES PATENT OFFICE.

WILLIAM D. MOUNT, OF SALTVILLE. VIRGINIA, ASSIGNOR TO NITROGEN PRODUCTS COMPANY. OF PROVIDENCE, RHODE ISLAND. A COEPOBATION OF RHODE ISLAND.

Application filed Ap'i126. 1918.

'To MU whom if muy mu r/W lo it known that I. umun l). MoUN'r, a 'citizen ot the l nitvil States 'osiding at Saltvillo. in the ronnty ot' h'nyth and Shiti' of Virginia. han jnV-ntwl cvitain now :nl lisi-tul lnp'ownonts` in \':iid-P'odnCinr Apparatns. ot' which the following' is a .specitivation.

Uno ot tht` ohj 'ts oi' sil inn-ntion is to provide noan` tor inlnving' a rvguhtwl llow of reavtion material through n H'tfli't oi' llll' liluto tlnonl that` proper 'c-zu'tion conditions nzy hr nnintainvl in said reti't. nothm' ohjvct is to provide z ronlination ot part\ through llli' internwliagv of which the tl'eatel material is Very vtliciontly voolrl and is presm'vol `i''o contanination hy :i' unt-il its` teinpc-ruhrv is su llllil^l1 l(\\`0l'l`*(ltl1l1t such rontanintion cannot ocmu' when through inatlvo'ten'o. or otherwise. ;i' ;zaim access to tho t'oatml mass'.

Thow ancl other ohjects of my invention will ho horeina'l'ti-r rvfvrred to and the no'vel vonhinations ot' means and elonn nts whorel v Hlllll ohjrc-ts may lw nttninul will ho more p'tivlnrly pointel ont in thappenlol olains.

In onof its aspvrt ny invontion (-onrv'nan inip'm'enent npoi'tlio appai'atns shown in the patont to John E. Bncher, No. 1.12058'3. (hlml llocenher l?) lili-l, in whi-h a t'ni'naris shown through a rvto't in ly gravity whihcurrent of nitrogen or nltl'olvmH gas is ranseil to ascend the volunn HircessiVeLY rooling thv bi'iqnets which haro travvrsvl the 'eziction zone, the niti-ngren being preheat-l iu so (loing. aml then paxing through or into the highly hontml portion of th(- 'otort to' read; with (-arlmnceous material and solinn cm'honate or tlnlihi in the vhnrgu to 'ton n tor FX: anple. soclinn vyanil.

ln opertig flll'lilt'vh ol' this description,

Specfcat'on of Letters Patent.

Pateted Feb. :L 1920.

Serial Ne. 230.876.

mnnto'od in removing the cyanized material t'a-oni the retorh owing to the hinding prop- 01`t ot' the cyanid t'orned.

The rha'ge while passing through the hnnt zone of the apparatns acquires a high Content of cyanitl, and when the cyanizel mass lHlHHOS into the cooling' zone below. the vynnil hanlons. with the result that the (hai-gi. initilly supplied in pieccs 01' preferahty in the t'o'n of hriquets, is united into a fairly solid column; the cyanicl acting as a hinler to nnitn the briqnets wherever they Inakp rontu-t with each other.

Thi` eolnnn is. of coni'so, filled with intvrstil'os when thi opvmtion is properly conducted: and the passage ot nit'ogen up the'vthrongh is hvnce not inaterially hinderol.

It is sntticiently rigicl and stron". howover to olti' a p'ollrn as how lihet to lisintegl'ate it. without too severely jar'ing the reto't, sinco heavy vontinuons viln'ntio' ohviously tends to `%hoi'ten the life of the appa'atns,

It is also desi'ahle not to nnnocessarily pnlvei-izo the cyanized material on account ot ohjcction to such powder during suhseqnunt opm'tions, The a 'paratns shown in the drnwings filfils these 'eqnirements and will no w he conside'ed in some detail In said drawings which 'form parts he'eof and in which like i'eference characters designate like parte in the respective views, I have shown a p'ete'red omhodinent of my invention; but. as I ani aware of various changes an\ modicatiom which may ho made heroin i\ ithmt (lopai'ting froni the spirit of said in.- vention. I (lPSlI'Q to ho limited only by the scopo of the clains, broadly inte'preted in the light ot' ny cliselosure.

Rehn-ring to the (l'awings:

Figni'e 1 iS a side elevaton of my improved cyanizing appa'atus; said elevation being pa'tly broken away to show details of i constrution.

Fig. 2 is a rem' View of the lower part of said appamtus; the View being taken from the line. II-II of Fig. 1.

Fg. 3 is a (letail section taken on the line ,l lI-fll of Fig. l; and,

Fig. 4 is a detail section taken on 'the line. lV---IV of Fig. 1.

The apparatis preferably comprises a rotort 1, of iron or other suitable material, which projects up through the fur-Ilace brick-work 2, and similarly extends down through the bottom platc 3; the prefcrahly cnlarged lower end 1' of said retort being soated in the mouth oi' the feedtablc casiug 4.

A gas-tight seul at the lower end of the retort is formed by compressing a packing of kieselgulr or other suitable material 5 around the outcr wall of said retort, by means of au annular casting 6.

The proferably coutinuously moving charge 7, is fed into the hopper 8, and por tion after portion thereof drops gradually and suocessively down through the preheating section of the retort until it enters the rcaction zone within the heated chamber 9; after which it is cooled somewhat in the enlarged section 1', before entering the casing 4.

The chemistry of the reaction need not be here further considered other than to state that in the preferrecl methbds of conducting the operation, thecharge is composed of brquets, the ingredients of which may be, for example, sodiun carbonate, pulverized coke, charcoal, or the like and finely divided iron. Nitrogen is supplied to this charge in the manner heroiuafter described. SO that at a temperature of. say, 1000 C., the carbon of the coke or charcoal is caused to unite with the free xiitrogen and With sodiun supplied lv the sodiun rarbonate, to form vauid. This reaction is prefer'ably etika-tal catalytically through the intermediacy of the iron, and by the time that a ::iron briqnet arrires at the bottom of the heat zone, it is normally highly eyanizod.

During their progress through the heat zone, the vanid present in the briquets is normally moltou, in large part. but as the Cyanizcd material cntcrs the cooling section 1', its fluid content'comnenccs to 'congeal; with the result that by the time such material enters the easing 4, it has set into a quite rigid column.

A rotary tablo 10 in this casing supports said column, and is provided with means for breaking oli briquets or fragments thi ren? from the bottom ot' the column to enable tlu charge in the retort to-g'raduallr dcseend.

The preferred (lt-vice for this purpose, is a 'star 11, having three points or arms and provided with. p \'ramidal teeth ll' to pickor pry oti' the' briquets without nuiterially pul- Veriziug; them. Said .star is loosely pivoted upon the uppvr surface of table 10, with its xis of rotation 12 em-ontri e to that ot' the table, as shown in l `i, 3. wherein the location ot' the shal't 13 which supports said tablo is indit'ated by a dotted circle.

Shai't 13 is suitably jourualod in hushings disposed respectively in the base or platr 14 and its yoke 16; the

niembor table shaft being driven by a. worm wheel 17, which in turn is driven by a worm 18 mounted on a shaft 19 which is preferably caused to 'evolve step by step by means of a ratchet wheel 20 and pawl 21. Wheel 20 is of course Secured to the shaft 19 and the pawl 21 is carried on an a'rm 22, pivoted on shaft 19, in a known fashion.

The shaft 19 is journaled in the yoke 16 and in a hearing 23 attached to one side of the hopper 24, which may Conveniently be made a part of the base plate 14.

The lopper 24 reccives the separate& briquets or fragments thereof, thns referahly pried off -from the charge, an delives them to a cooling tank 25. This tauk is preferably, what may he terned, flat lmug quite narrow in proportion to broadth and depth, as shown in Fgs. 1 and 2; so that it afl'ords a Very extensive surface', in proportion to its Volume or cubical content, to permit of air or water cooling and cooling' by ral-iation.

It may be here noted that the material to be cooled is a, relatively poor mnductor of het; but by thus providing a large fiat tank, the distance from the most interiorly disposed point in the mass to be cooled, to the exposed cooling surface need not be over two or three inches. The tank is also preferably tapered toward the bottom, as shown, to still further rednce said distanca with the result, that the temperature of the material drawn 'from valve 26 at the lower end of said tank is normally but very little above that ot' the surrounding atuosphere.

In the constructou .given by way of illustratiom a hearing brat-ket 27 is mounted upon one side of the tanlc; and has journaled therein a sha't't 28, one` end of which rarrios an ecrentric 29 and the other end a sprookot wheel 30 othe like A I'od 31 connerts the errentric strap 29' with the arm 22, so that as the shaft 28 is rotated by the wheel :50. rod to cause the pawl 21 to step the ratchet wheel around wherehy to cause a coi-responding step by step but much slower rof tary uotion ot' the feed tahle.

As this action takes place. on acrount of the errentricity of the star 11 with respect to said table, the teeth 11' are eausod to pow-ri'ully pry or pi'k tragneuts from the column above the table: first one tooth coming into play and thon' another, or. at times, )ossill two of the teeth, simultaneously breaking oti fragments.

A further advantage in ths ecceutrically uounting a loosely piroted toothed element upon th( rotary table. is that the change is prevented from idly' rotating in its retort: as it is apt. to do where th(` table itself can ries the teeth and has its nxis o-incident with that of a cylindrical retort.

its

The tank preterahly has a Capacity two or three tin es that of the retort, when air cooled shown.

Air is exeluded from the tank and of course froni the casng 4: and retort, to provent the oxidntion of the eyanid formed. to oyanate; and for this and other reasons hereinafter noted, nitrogen is introdueed into the bottom ot' the tenk through a pipe 3:2; the flow ot' gas being controlled. by means of valve 33.

The niti-egon eurrentfiows up through the tank, between the interstices of the briquets or charge tragnents, aiding in cooling said fragments and in turn being preheated by contact with them.

By the time that it enters the casing -l and 'passes thence through the laternlly unsupported walls of the' rigid briquet column, into reto't section 1', it is quite not; but still of course below the melting point of eyanid. As it therea''ter traverses the poi-es and interstices of the hriqueted eharge, it is gradually raised to the reaetion tempe ature, while again in turn aiding in qooling the descending cyanized eharge, to cause any liquid present in the latter to congeal or solidify.

The vnlve 20 ut the lower end of the cooling reeeptncle, is preferably a one Way k. as shown in Fig. 4; having therein a poeket :26' so that when it is, for example, eontinuously rotated, this poeket is alternately filled and emptied at every revolution.

Preterahly this vulve is driven slowly hy means of a sproeket' and chain drive; shutt 19 having feathered on one end a eluteh 34 which when operatirely disposed causes said shatt to drive a sproehet wheel 35, which in turn aetuates a chain 3(' to drive a sproeket wheel 37 mounted on a truunion 68 of said valve 26 Clutch is thrown to cause valve 20 to rotzte, a receiving can 39 is placed in position below the valve casing 40.

The general operation of the appzu'atus may now be briefly reviewed.

Assuning that the retort is charged with,

briquets and that its beat-zone section has attained the proper temperature, the supply of hoat being maintained by the flow of hot gases through the furnac'e in the direction of the arrows; the charge will. then grad ually move down through the retort each briquet being first pre-heated by the ascending gaseous reaction products.

Thereafter each brquet will, in turn he eyanized and then pass into the cooling seetion 1", where its liquid Content Will congeal. In so doing the .briquets in said sec tion will adhere together to form a rather rigid structure, which will he sustained by therotating table and will inturn snstain the remainder of the charge in the 'etort.

Normally, ot' course, before the- The laterally self-sustaining character ot' this briquet structure permits the nitrogen flowing through the casing 4, to gain t'i-ee access to the interier of the column, from all sides of the letter and thenee up to the reaction zone.

The rotation of the table eauses the teeth and other ahrading parts of the eccentrically pivoted star or cutter to bite off pieces from the bottom of the eolumn, and these loose fragmente are gradually worked oti." of the table and fall through the hopper 24 into the cooling' tenk; there being no lateral supports zround the lower end ot the eolunn to hinder this movement. Pulverimtion ot' the briquet material should preferihly he avoided to favor the sulsequent reeovenv of the eyanogen compound by an extracting operation.

Nitrogen supplied from pipo 32 cools the briquets in the cooling tani( and thereafter lowers the temperature of those in the ras ing 4 and retort section 1'; the nitrogen 'being reheated thereby.

h eznwhite the eharge in the retmt is renewed so s to maintain said retort substantially full; and it the reaetion gases be not t'ollectted as they emerge from the hopper 8. they will burn at this point.

It has been found most convenient and practieable however. to make no attempt. to reeover these gzises the hopper ti heiug left open to pernit of the tree introduction oi' the charge.

The substa'tially cold hriquets in the lower end of the tank are Withdrawn. from time to time or eontinuously, as desiretl. and especially in the latter mode ot' operation, is it desirable to provide some means. such :s the. vnlve 26 and its assoeiated parts. to prevent wastage of the nitrogen supplied to the retort; or, even worse, such an outflow ohoth cooled briquets and nitrogen from the receptacle as might tend to create a backword flow of nitrogen not only through the cooling tank, but even down- Wa'dly through the retort; since in such ease free utmospherio oxygen would also flow Clown from the open upper end of said I'etort.

'I may add, that I have found it advantageous to thus supply nitrogen to the bottom of the cooling' reeeptacle in order to more efliciently and eeonoically cool the briquets while at the same time conservinr much of the heat ot' which they are deprive&

Ii eonlusiou I desire to point out that my invention not only eontemplates the novel apparatus above described: but nlso themethod of fixing niti-egon made possible by this or an equivalent eonstrction. This method is. in certain of its aspeets. especially eoncerned With the turning to ad- Yuntage in several ways. of what otherwise lDO would tend to give rise to considerable trouble in the nitrogen fixing operation. I refet' here more particularly to the chilling and congealing ofthe cyanid formed, following its removal from the heat zone; which congelation, above noted, has been fa ored under controlled conditions and uulized to aid in the subsequent preparation of the cyanized material for the extracting operation.

Having thus described my invention, What I claim is: r

1. In apparatus for trcating free n-itrogen to efl'ect the fixation thereof, the combination of a furnace having thcrein a cyanizing retort, with means to cfi'ect a g'adual movement of cyanized material out of said retort at a temperature below that at which the cynaid formed congeals, said* means including a toothcd device for breaking ofl' fragmente of said cyanized material and power-driven means for actuating said device.

In apparatus for treating free nitrogen to cfl'ect the fixation thereof, the combinetion of a fu'nace having therein a cyanizing retort, With means to efiect a gradual movement of cyanized material out of said retort in the form of a substantially rigid column, said means including a movably mounted device for picking to fragmente the said material at the base of the column and power-driven means for acutating said device.

3. In apparatus for treat ng free nitrogcn to efi'ect the fixation thereof, the comlination `of a furnace having therein a cyanizing retort, with means to efl'ect a gradual movement of cyanized material away from the heat zone of said retort in the form of a. substantially ,rigid porous column, said means including a rotarily mounted device for pickin to pieces and progressively removing said material at the base of the column, and means to supply nitrogen directly to portions of said rigid column as said portions become accessible to said nitrogen by their movement away from the walls of said retort.

4. In apparatus for treating free nitrogen to efl'ect the fixation thcreof, the combination of a furnace havingtherein a cyanizing reto't, with means to efl'ect a gradual movement of cyanized material out of said retort at a temperature below that at which the cyanid formcd congals, said means including a toothed devce for breaking ofl' fragmente of said cyanized material, a rotary table upon which said device is loosely pivoted and means to drive said table rctarily, the axis of rotation of the tahlebeing eccentric to that of said device.

5. In apparatus for treating fre nitrogen to effect the fixation thereof, the mbination of a furnace having ther-ein a cyanizing retort, with means to efl'ect a gradual movement of cyanized material out of said retort at a temperature below that at which the cyanid formed congeals, said means including a toothed devoe for breaking ofl' fragmente of said cyanized material, a rotary table upon which said device is loosely pivoted and means to drive said table rotarly.

6. In apparatus for treating free nitrogen to el'ect the fixation thereof, the co'mbination of a frnace having therein a cyanizing retort, with means to efl'ect a gradual movement of cyanized material out of said retort at `a temperature below that at which the cyanid formed congeals, said means including a rotary table to support said material, neans to drive said table and means to cut away fragmente from the bulk of said material as the material of which said fra ments are eomposed approaches said mbi.

7. In apparatus for treating free nitrogen to effect the fixation thereof, the combineton of a furnace havin therein a cyanizing retort, wthi'neans to e ect a gradual movement of cyanized material out of said retort at a temperature below that at which the cyanid formed congeals, said means including a rotary table to support said material,

means to drive said table and a toothed star pivoted upon said table eccentrically with respect to the table axis, to enable parte of said star to cut away fragmente from the bulk of said material as the material of which said fra ents are composed approaches said'ta' le. v

8. In apparatus for treating free nitrogen to efi'ect the fixation thereof, the combine- 'tion of a cyanizing retort, means co-acting with gravity to cause a general but substantially continuous movement of cyanized material out of said retort, means to reduce said material to fragments, a fiat cooling tank to receive said fragments, and means to supply free nitrogen to said tank and retort.

9. In apparatus for treating nitrogenous materials, the combination of a retort in which free nitrogen is first combined with other materialsto form a fluid nitrogenous compound, and` in which retort, further, said compound is subseqnently seliclified, with means to co-act with gravity to eifect a gradual extrusion of solidified material from said retort while breaking said material into fragmente, means to receive and cool said fragments, means to supply free and relatively cool nitrogen to the mass of said fragmente in' said cooling means, to aid in lowerin the temperature of said mass while pre eating said ijtrogen, and

pl'ovisions to control the movement of cooled fragmente out of said cooling means. 10. In apparatus for treating nitrogenous the oibimtion oi' zi i'oto't iii which 'free iit'ogei is first coiibied With otlur outcriuh; to form u [luid it'ogenous i-opooiti ;oui in which 'eto-t, further, said (-m'pouid is sulmoqueny solitiiiied, 'with roboy luhio Lo support the cha'ge iii :aiLi otom lmdll-j, cur'iod by said tubim for h'ouhiog; up :solhliied iiatei'iul exti'uded f'o said 'etq''t, and means to 'otute said tablo step by step.

11. Iu uppurztus for t'eatig nitrogeious hmm-ini& the uouhiuton of a i'etort in which free. nitrogen io first combined with other'uuh i'iuls to oroi EL fluid iitrogeous ('0il!]lUllIHi anii .ill which 'eto'., further, said ,-n p,o1\ subsequetl' soiidiied, with a l'Uill' table h support the ch rge in said i't'tol't, menus, cui''ieii by said table, 1 01.' breaking up soliciified iiaterial cxt'uded from said i'eto't, u Wom and wheel drive 01' :said table, and step by step miting means for opcruting said (h'ive.

12. Thu gomhination of u vertical i'eto't, with !11021135 't'oheating the smile, a unsing connected io the lower end of said 'etoi't, liiL'CiiillliSlH in Saiti casing, to co nct with 'i'zn'ihv to {cod the chz'ge fmin said` reto't, iieons to drive said IHBCillIiiSli, u cobiing -cposito'y to receive the material removed fron ai i i'etoi't., meiuis to control the move ment of (zooied material out oi' said 'epositou\ and means to uppl'y H gas to be t'euted in said TL'tUi'il to sfiid '0psit0 nt i\ point mi` iiv bottoi tha-yeni 1 1. in uppui'ls i'm' t'euting free ii tro- ;ren to vi'eci the fixation thoi'eof, the conibinzttion oi' u forum-e having thei-ein u Cyaniizing i-vlo'i` with means to efl'ect u gruduui uowinuni oi' eynizml material 0nt oi' said rvto' ut :i teupc'utu'e below (hat. ai. which the cyun'ui form-d congeuls, said means in (jhliillg' zi 'otai'y tubhto support Hoh\ ma tv'iz l, means to d'ivo said table and u pickir g devic'e pivotad upon sziid table macent icziliy with respect to the table nxis, to

enable penis of said device to pry away fi'g menus from the buik of said material us the mute'iui of which said frgnents' aire composed approaches said table.

14. In combinutinn, ai fu'nace having jn'ozlciies sahi support.

15. In combinuton i'u'num having tho'oin a l'UiUl't i whi h uonutitovnt oi' the n'iotoriul Uilitl'gilij i'i'oo said 'oto't it'iih to act udhesively upon (-ooiim with menus to efleci u gi'mhizl inowoet of" Hlhi ouv 'iii out of said roto't u( o hropvralui'v ut which said nuto'iai is 'lliilt'l'mi together by said constituent thcreoi', said menus inohul ing 'ota'iiy mouutod supporting menus foi- ;aid mutei'inh ivuu` to (i'ivc Hnid hppmt ing ieans i'otai'iiy und menus 'i'op'ying oti' f'gne'its from the buik of Suid nae'iai :s ithe motorin] of which said frog nichts are couposed zipp'ou-hwi said suppmtiug nie-uns.

16. in combinuiion. 2\ i'nrzco having' the'uin zi I'ctm't i' which :l (tonstituet oi' {ho oiuteyiu] ei e'ging' from sahi retort tends to :ost ndhesiveiy upon ('()()ii1) with menus io efect :i gi'zuhuli iowoont of sniii material out ot: siil reto't nt a tempo'utuo at which szil material is mlhc'cd together by nuhi onstituoit thmi-ot .said HIWUH including 'otz'iiy mountoii support l'o' szial ntu'iui. and :i device pivomiiiy iouitml upon sahi support 'Fol' piving oti' sogno-otr; f'ou thu bnik of suit! motorin\ us th( inuto'izi of which suiil f'agnonls uri coposvd :p p'o'achos said support. 4

In testiony Wht'eof I how. :flixod my Signature in the presence oi' two witnesses. v VVILLIAM D. MOUNT.

F. WATSON,

M. ARCHER.

W itnesses: JAMES JAMES 

